Reaktion #2512232

Reaktionsgleichung

(S)—N-benzyl-α-methylbenzyl-amine

(±)(6S)-2-oxobicyclo[3.1.0]hexane-6-carboxylic acid

ethanol

→

salt

(+)(6S)-2-Oxobicyclo[3.1.0]hexane-6-carboxylic acid N-benzyl-α-methylbenzylamine salt

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONUpon dissolution
2. 2
   Temperaturto cool optionally
3. 3
   Sonstigeby seeding at 52° C
4. 4
   Sonstigethe crystals are collected
5. 5
   Waschenwashed with 6:1 ethyl acetate
6. 6
   SonstigeDrying in vacuo

Vorschrift

To a solution of crude (±)(6S)-2-oxobicyclo[3.1.0]hexane-6-carboxylic acid (11.9 g, 84.9 mmol, assume 100% potency) in 119 mL of 6:1 ethyl acetate:ethanol at reflux is added 18 g (85.1 mmol) of (S)—N-benzyl-α-methylbenzyl-amine. Upon dissolution, the mixture is allowed to cool optionally followed by seeding at 52° C. Upon cooling to room temperature and stirring an additional 13.5 h, the crystals are collected and washed with 6:1 ethyl acetate:ethanol (2×48 mL). Drying in vacuo gave 10.8 g (36%, 77% de) of the resolved salt as a solid.

Quelle